WO2015008883A1 - Multi-cell type electrospinning tube and method for producing nanofibers using same - Google Patents

Multi-cell type electrospinning tube and method for producing nanofibers using same Download PDF

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Publication number
WO2015008883A1
WO2015008883A1 PCT/KR2013/006476 KR2013006476W WO2015008883A1 WO 2015008883 A1 WO2015008883 A1 WO 2015008883A1 KR 2013006476 W KR2013006476 W KR 2013006476W WO 2015008883 A1 WO2015008883 A1 WO 2015008883A1
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electrospinning
cell type
tube
electrospinning tube
nanofibers
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PCT/KR2013/006476
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French (fr)
Korean (ko)
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김학용
남기택
정진원
전경수
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전북대학교산학협력단
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Priority to PCT/KR2013/006476 priority Critical patent/WO2015008883A1/en
Publication of WO2015008883A1 publication Critical patent/WO2015008883A1/en

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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/18Formation of filaments, threads, or the like by means of rotating spinnerets
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin

Definitions

  • the present invention relates to a multi-cell type electrospinning tube used as a mechanism for discharging a polymer spinning solution when producing nanofibers by an electrospinning method, and a method of manufacturing nanofibers using the same.
  • an electrospinning tube composed of a plurality of discharge cells is defined as a "multi-cell type electrospinning tube”.
  • the conventional electrospinning apparatus electrospins the spinning liquid through a fixed nozzle, the electrospinning is performed only depending on the electrostatic force, so that the discharge amount per nozzle unit nozzle per unit time is very low to 0.01g, resulting in low productivity. Difficult problems, nozzle replacement and cleaning are very complicated and cumbersome.
  • the production of nanofibers through electrospinning is 0.1g to 1g per hour as described in Nanotechnology 2006. VOL 17, 1123 (D.H.H. Renecker et al.) And the solution discharge rate is very low, 1.0mL to 5.0mL per hour.
  • Another conventional electrospinning apparatus is an electrospinning apparatus for electrospinning the spinning liquid (polymethyl methacrylate solution dissolved in chlorobenzene) using only a centrifugal force by using a cylinder rotating at a high speed of 3,000 rpm or more.
  • Another conventional electrospinning apparatus is a small electrospinning apparatus for supplying a polyvinylpyrilidone solution while applying a high voltage to a conical container rotating at 50 rpm to simultaneously perform electrospinning without a nozzle using electrostatic force and centrifugal force.
  • the conventional electrospinning apparatuses can improve the output per unit time in a nozzleless form by utilizing centrifugal force and electrostatic force, it is difficult to continuously produce the spinning liquid in the conical container, and the lower part of the conical container There is a problem that the collector is located in the spinning liquid is not in the form of fibers, but drops into a solution state (hereinafter referred to as "drop generation phenomenon").
  • the conventional electrospinning method has a problem in that the production of nanofibers per unit hole is very low and the nozzle cleaning is cumbersome by using the nozzle.
  • the problem of the present invention is high productivity per unit time during electrospinning, can eliminate the trouble of the conventional nozzle replacement and nozzle cleaning, can effectively prevent the occurrence of drop, multi-cell capable of continuous production of nanofibers It is to provide a type electrospinning tube.
  • Another object of the present invention is to provide a method for producing nanofibers using the multi-cell type electrospinning tube.
  • a multi-discharge cell (S) composed of a plurality of discharge cells (S) having one type selected from a circular rod and a polygonal rod
  • a cell type electrospinning tube Provided is a cell type electrospinning tube.
  • a plurality of discharge cells having one type selected from a circular bar and a polygonal bar as the electrospinning tube ( A multi-cell type electrospinning tube T including S) is used, and the multi-cell type electrospinning tube T is rotated during electrospinning.
  • the present invention improves productivity per unit time by increasing the point at which nanofibers are formed during electrospinning by spinning a polymer spinning solution into a rotating multi-cell type electrospinning tube so that electrostatic and centrifugal forces can be used together, and nozzle replacement and cleaning Eliminates the hassle, effectively prevents the occurrence of drop, and continuous supply of spinning solution has the advantage that the continuous production of nanofibers.
  • 1 to 2 are schematic top views of one example of a multi-cell type electrospinning tube according to the present invention.
  • FIG. 3 is a perspective schematic view of the discharge cell S shown in FIG. 1;
  • Figure 4 is an electron micrograph of the nanofiber web prepared in Example 1 of the present invention.
  • the multi-cell electrospinning tube according to the present invention has a plurality of discharge cells (S) having one type selected from circular bars and polygon bars as exemplarily shown in FIGS. 1 to 3. Characterized in that consists of.
  • FIG. 1 is a plan view of a multi-cell type electrospinning tube of the present invention in which the discharge cell S is in the form of a hexagonal rod
  • FIG. 2 is a bone in which the discharge cell S is in the form of an octagonal rod.
  • a plan view of a multi-cell type electrospinning tube of the invention, and FIG. 1 is a perspective schematic view of a discharge cell S in the form of a hexagonal rod of FIG. 1.
  • the height h of each of the plurality of discharge cells S is the same.
  • the height h is not constant, it is not preferable to maintain the shape of the electrospinning tube T composed of a plurality of discharge cells S and to uniformly supply the polymer spinning solution.
  • Discharge cells (S) in the form of a polygonal bar is preferably a triangular to hexagonal shape having three to 16 corner angles, more preferably hexagonal or octagonal.
  • the plurality of discharge cells S may be all identical to each other, all may be different from each other, some may be the same, and others may be different.
  • the plurality of discharge cells S may all have the same size, all may be different from each other, some may be the same, and others may be different.
  • the size and height h of the discharge cell S are not particularly limited.
  • the multi-cell type electrospinning tube according to the present invention is supported by an electrospinning tube support, and it is preferable that the polymer spinning solution is stably supplied through a distribution plate located at the bottom of the electrospinning tube.
  • the electrospinning tube support may be, for example, a cylindrical structure having a diameter of 3 mm or more.
  • the electrospinning tube is provided with one type selected from a circular rod and a polygonal rod as the electrospinning tube so that the electrospinning and centrifugal force can be used together when the polymer spinning solution is electrospun through an electrospinning tube to produce nanofibers.
  • a multi-cell type electrospinning tube T including a plurality of discharge cells S is used, and the multi-cell type electrospinning tube T is rotated during electrospinning. .
  • the rotation speed of the multi-cell type electrospinning tube T is preferably set to 50 rpm or more, more preferably 50 to 500 rpm.
  • the number of rotation of the multi-cell type electrospinning tube (T) is different depending on the diameter, shape, number, arrangement number and arrangement method of the cell (S) formed in the electrospinning tube (T), the present invention
  • the rotation speed is not particularly limited.
  • Electrospinning was carried out through a multi-cell type electrospinning tube T arranged in a honeycomb structure in an electrospinning tube T having an inner diameter of 50 mm.
  • the multi-cell type electrospinning tube (T) was rotated at 200 rpm during electrospinning.
  • the nanofibers were prepared by contacting the nanofibers electrospun through the multi-cell electrospinning tube T on a rotating collector.
  • the discharge amount per one of the multi-cell type electrospinning tube (T) is 0.5g / min, significantly improved compared to the discharge amount of the conventional electrospinning apparatus.
  • the electron micrograph of the prepared nanofiber web was as shown in Figure 4 and no drop occurred.
  • the average diameter of the prepared nanofibers was 200 nm.
  • Electrospinning was carried out through a multi-cell type electrospinning tube T arranged in a honeycomb structure in an electrospinning tube T of mm.
  • the multi-cell type electrospinning tube (T) was rotated at 200 rpm during electrospinning.
  • the nanofibers were prepared by contacting the nanofibers electrospun through the multi-cell electrospinning tube T on a rotating collector.
  • the discharge amount per one of the multi-cell type electrospinning tube (T) is 0.55g / min, significantly improved compared to the discharge amount of the conventional electrospinning apparatus.
  • the average diameter of the prepared nanofibers was 210 nm.
  • discharge cells (S) having a hexagonal rod shape shown in FIGS. 1 and 3 and having a length of 6 mm on one side are shown.
  • 2 is arranged in a honeycomb structure in an electrospinning tube T having an inner diameter of 50 mm so that the discharge cells S having a length of 4 mm on one side are alternately repeated. It was electrospun (discharged) through the cell type electrospinning tube (T).
  • the multi-cell type electrospinning tube (T) was rotated at 200 rpm during electrospinning.
  • the nanofibers were prepared by contacting the nanofibers electrospun through the multi-cell electrospinning tube T on a rotating collector.
  • the discharge amount per one of the multi-cell type electrospinning tube (T) is 0.6g / min, significantly improved compared to the discharge amount of the conventional electrospinning apparatus.
  • the average diameter of the prepared nanofibers was 205 nm.
  • the present invention is used as a device for electrospinning high quality nanofibers with high productivity.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The multi-cell type electrospinning tube according to the present invention comprises a plurality of discharge cells (S) having a circular rod shape or a polygonal rod shape. The method for producing nanofibers according to the present invention is characterized by: when producing the nanofibers by electrospinning a polymer spinning solution by means of an electrospinning tube, using as the electrospinning tube a multi-cell type electrospinning tube (T) comprising a plurality of discharge cells (S) having a circular rod shape or a polygonal rod shape; and rotating the multi-cell type electrospinning tube (T) during electrospinning. By spinning the polymer spinning solution by means of the rotating multi-cell type electrospinning tube so as to use both electrostatic force and centrifugal force, the present invention provides the advantages of improving productivity per unit time by increasing points where the nanofibers are formed during electrospinning, removing the inconvenience of replacing and cleaning nozzles, effectively preventing the occurrence of a drop phenomenon, and continuously producing the nanofibers by continuously supplying the spinning solution.

Description

멀티-셀 타입 전기방사용 튜브 및 이를 이용한 나노섬유의 제조방법Multi-cell type electrospinning tube and manufacturing method of nanofibers using the same
본 발명은 전기방사 방식으로 나노섬유를 제조할 때 고분자 방사용액을 토출하는 기구로 사용되는 멀티-셀(Multi-cell) 타입 전기방사용 튜브 및 이를 이용한 나노섬유의 제조방법에 관한 것이다.The present invention relates to a multi-cell type electrospinning tube used as a mechanism for discharging a polymer spinning solution when producing nanofibers by an electrospinning method, and a method of manufacturing nanofibers using the same.
이하, 본 발명에서는 다수개의 토출용 셀(Cell)들로 이루어져 있는 전기방사용 튜브를 "멀티-셀 타입 전기방사용 튜브" 라고 정의한다.Hereinafter, in the present invention, an electrospinning tube composed of a plurality of discharge cells is defined as a "multi-cell type electrospinning tube".
종래 전기방사장치들은 대한민국 등록특허 제10-0420460호 등에 게재된 바와 같이 방사액을 토출하는 기구로 고정된 원형 막대 형태인 노즐(Nozzle)을 주로 사용되어 왔었다.Conventional electrospinning apparatuses have been mainly used as a nozzle (Nozzle) in the form of a fixed circular rod as a mechanism for discharging the spinning liquid, as disclosed in Republic of Korea Patent No. 10-0420460.
그러나, 상기 종래 전기방사장치들은 고정된 노즐을 통해 방사액을 전기방사(토출)하기 때문에 정전기력에만 의존하여 전기방사가 실시되어 단위시간당 노즐 단위홀당 토출량이 0.01g 수준으로 매우 낮아 생산성이 떨어져 결국 양산화가 어려운 문제점과, 노즐 교체 및 청소가 매우 복잡하고 번거로운 문제점 등이 있었다.However, since the conventional electrospinning apparatus electrospins the spinning liquid through a fixed nozzle, the electrospinning is performed only depending on the electrostatic force, so that the discharge amount per nozzle unit nozzle per unit time is very low to 0.01g, resulting in low productivity. Difficult problems, nozzle replacement and cleaning are very complicated and cumbersome.
일반적으로 전기방사를 통한 나노섬유의 생산량은 나노테크놀리지 2006. VOL 17, 1123(D.H.H. Renecker 등)에 기재된 바와 같이 시간당 0.1g 내지 1g 수준이고 용액 토출량은 시간당 1.0mL 내지 5.0mL 수준으로 매우 낮다.In general, the production of nanofibers through electrospinning is 0.1g to 1g per hour as described in Nanotechnology 2006. VOL 17, 1123 (D.H.H. Renecker et al.) And the solution discharge rate is very low, 1.0mL to 5.0mL per hour.
또 다른 종래의 전기방사장치로는 3,000rpm 이상으로 고속회전하는 원통을 이용하여 상기 원통 내에 투입된 방사액(클로로벤젠에 용해된 폴리메틸메타아크릴레이트 용액)을 원심력만을 이용하여 전기방사하는 전기방사장치가 나노레터(Nano Letters)에 발표한 논문(Nano Letters, 2008, Vol 8, No.4, 1187-1191)에 게재되어 있다.Another conventional electrospinning apparatus is an electrospinning apparatus for electrospinning the spinning liquid (polymethyl methacrylate solution dissolved in chlorobenzene) using only a centrifugal force by using a cylinder rotating at a high speed of 3,000 rpm or more. Is published in Nano Letters (Nano Letters, 2008, Vol 8, No. 4, 1187-1191).
또 다른 종래의 전기방사장치로는 50rpm으로 회전하는 원추형 용기에 고전압들을 걸어주면서 폴리비닐피릴리돈 용액을 공급하여 정전기력과 원심력을 동시에 이용하여 노즐 없이 전기방사를 실시하는 전기방사장치가 2010년 스몰(Small)지에 게재된 논문(Small, 2010 Vol 6, 1612-1616 : Nanzhou 대학 Jinyuan Zhou)에 기재되었다.Another conventional electrospinning apparatus is a small electrospinning apparatus for supplying a polyvinylpyrilidone solution while applying a high voltage to a conical container rotating at 50 rpm to simultaneously perform electrospinning without a nozzle using electrostatic force and centrifugal force. (Small, 2010 Vol 6, 1612-1616: Jinyuan Zhou, Nanzhou University).
그러나, 상기 종래의 전기방사장치 들은 원심력과 정전기력을 활용하여 노즐이 없는 형태로 단위시간당 생산량을 향상시킬 수는 있지만 상기 원추형 용기내에 방사액을 연속 공급하여 연속 생산이 어려운 문제점과, 상기 원추형 용기 하부에 컬렉터가 위치하여 방사액이 섬유형태가 아니라 용액상태로 떨어지는 현상(이하 "드롭발생 현상"이라고 한다)이 일어나는 문제점이 있었다.However, although the conventional electrospinning apparatuses can improve the output per unit time in a nozzleless form by utilizing centrifugal force and electrostatic force, it is difficult to continuously produce the spinning liquid in the conical container, and the lower part of the conical container There is a problem that the collector is located in the spinning liquid is not in the form of fibers, but drops into a solution state (hereinafter referred to as "drop generation phenomenon").
또 다른 종래의 전기방사장치로는 국제공개(WO)2005-073441호 등에 게재된 바와 같이 다량의 노즐을 노즐 판상에 배열하여 전기방사하는 시스템에 대한 방식 등도 이미 잘 알려져 있다.As another conventional electrospinning apparatus, a method for an electrospinning system in which a large number of nozzles are arranged on a nozzle plate as disclosed in WO 2005-073441 is well known.
그러나 상기 종래의 전기방사 방식은 단위 홀당 나노섬유의 생산량이 매우 낮고 또한 노즐을 사용함으로써 노즐의 청소 등이 번거로운 문제점이 있었다. However, the conventional electrospinning method has a problem in that the production of nanofibers per unit hole is very low and the nozzle cleaning is cumbersome by using the nozzle.
본 발명의 과제는 전기방사시 단위시간당 생산성이 높고, 종래 노즐 교체 및 노즐 청소에 따른 번거로움을 해소할 수 있고, 드롭발생현상도 효과적으로 방지할 수 있고, 나노섬유의 연속생산이 가능한 멀티-셀 타입 전기방사용 튜브를 제공하는 것이다.The problem of the present invention is high productivity per unit time during electrospinning, can eliminate the trouble of the conventional nozzle replacement and nozzle cleaning, can effectively prevent the occurrence of drop, multi-cell capable of continuous production of nanofibers It is to provide a type electrospinning tube.
본 발명의 또 다른 과제는 상기 멀티-셀 타입 전기방사용 튜브를 이용하여 나노섬유를 제조하는 방법을 제공하는 것이다.Another object of the present invention is to provide a method for producing nanofibers using the multi-cell type electrospinning tube.
이와 같은 과제들을 달성하기 위해서, 본 발명에서는 전기방사시 고분자 방사용액을 토출하는 기구로서, 원형 막대 및 다각형 막대 중에서 선택된 1종의 형태를 구비하는 다수개의 토출용 셀(S)들로 구성된 멀티-셀 타입 전기방사용 튜브를 제공한다.In order to achieve the above problems, in the present invention, as a mechanism for discharging the polymer spinning solution during electrospinning, a multi-discharge cell (S) composed of a plurality of discharge cells (S) having one type selected from a circular rod and a polygonal rod Provided is a cell type electrospinning tube.
또한, 본 발명에서는 고분자 방사용액을 전기방사용 튜브를 통해 전기방사하여 나노섬유를 제조할 때 상기 전기방사용 튜브로서 원형 막대 및 다각형 막대 중에서 선택된 1종의 형태를 구비하는 다수개의 토출용 셀(S)들을 포함하는 멀티-셀 타입 전기방사용 튜브(T)를 사용하고, 전기방사시 상기 멀티-셀 타입 전기방사용 튜브(T)를 회전시켜 준다.In addition, in the present invention, when producing a nanofiber by electrospinning a polymer spinning solution through an electrospinning tube, a plurality of discharge cells having one type selected from a circular bar and a polygonal bar as the electrospinning tube ( A multi-cell type electrospinning tube T including S) is used, and the multi-cell type electrospinning tube T is rotated during electrospinning.
본 발명은 정전기력과 원심력을 함께 이용할 수 있도록 고분자 방사용액을 회전하는 멀티-셀 타입 전기방사용 튜브로 방사함으로써 전기방사시 나노섬유가 형성되는 포인트를 늘려서 단위시간당 생산성이 향상되고, 노즐 교체 및 청소의 번거로움을 해소하고, 드롭발생현상도 효과적으로 방지하고, 방사액을 연속공급해서 나노섬유를 연속생산이 가능한 장점이 있다.The present invention improves productivity per unit time by increasing the point at which nanofibers are formed during electrospinning by spinning a polymer spinning solution into a rotating multi-cell type electrospinning tube so that electrostatic and centrifugal forces can be used together, and nozzle replacement and cleaning Eliminates the hassle, effectively prevents the occurrence of drop, and continuous supply of spinning solution has the advantage that the continuous production of nanofibers.
도 1 내지 도 2는 본 발명에 따른 멀티-셀 타입 전기방사용 튜브 일례의 평면 개략도.1 to 2 are schematic top views of one example of a multi-cell type electrospinning tube according to the present invention;
도 3은 도 1에 도시된 토출용 셀(S)의 사시 개략도.3 is a perspective schematic view of the discharge cell S shown in FIG. 1;
도 4는 본 발명의 실시예 1로 제조한 나노섬유 웹의 전자현미경 사진.Figure 4 is an electron micrograph of the nanofiber web prepared in Example 1 of the present invention.
* 도면 중 주요부분에 대한 부호설명* Code description for main parts of the drawings
T : 멀티-셀 타입 전기방사용 튜브T: Multi-cell type electrospinning tube
S : 멀티-셀 타입 전기방사용 튜브를 구성하는 토출용 셀S: Discharge cell constituting the multi-cell type electrospinning tube
h : 멀티-셀 타입 전기방사용 튜브를 구성하는 토출용 셀의 높이h: Height of the discharge cell constituting the multi-cell type electrospinning tube
이하, 첨부한 도면 등을 통하여 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
먼저, 본 발명에 따른 멀티-셀 전기방사용 튜브는 도 1 내지 도 3에 예시적으로 도시된 바와 같이 원형 막대 및 다각형 막대 중에서 선택된 1종의 형태를 구비하는 다수개의 토출용 셀(S)들로 구성되는 것을 특징으로 한다.First, the multi-cell electrospinning tube according to the present invention has a plurality of discharge cells (S) having one type selected from circular bars and polygon bars as exemplarily shown in FIGS. 1 to 3. Characterized in that consists of.
도 1은 토출용 셀(S)의 형태가 6각형 막대 형태인 본 발명의 멀티-셀 타입 전기방사용 튜브의 평면도 이고, 도 2는 토출용 셀(S)의 형태가 8각형 막대 형태인 본 발명의 멀티-셀 타입 전기방사용 튜브의 평면도이고, 도 1은 도 1의 6각형 막대 형태인 토출용 셀(S)의 사시개략도 이다.1 is a plan view of a multi-cell type electrospinning tube of the present invention in which the discharge cell S is in the form of a hexagonal rod, and FIG. 2 is a bone in which the discharge cell S is in the form of an octagonal rod. A plan view of a multi-cell type electrospinning tube of the invention, and FIG. 1 is a perspective schematic view of a discharge cell S in the form of a hexagonal rod of FIG. 1.
상기 다수개의 토출용 셀(S)을 각각의 높이(h)는 서로 동일하다. 상기 높이(h)가 일정하지 않을 경우 다수개의 토출용 셀(S)로 구성된 전기방사튜브(T)의 형태를 유지해주고 고분자 방사용액을 균일하게 공급해 주기 어렵게 되어 바람직하지 못하다.The height h of each of the plurality of discharge cells S is the same. When the height h is not constant, it is not preferable to maintain the shape of the electrospinning tube T composed of a plurality of discharge cells S and to uniformly supply the polymer spinning solution.
상기 다각형 막대 형태인 토출용 셀(S)은 모서리각이 3개 ~ 16개인 삼각형 ~ 십육각형 형태인 것이 바람직하며, 보다 바람직하기로는 육각형 또는 팔각형인 것이 좋다.Discharge cells (S) in the form of a polygonal bar is preferably a triangular to hexagonal shape having three to 16 corner angles, more preferably hexagonal or octagonal.
상기 다수개의 토출용 셀(S)들은 형태가 모두 서로 동일할 수도 있고, 모두 서로 상이할 수도 있고, 일부는 동일하고 나머지 일부는 상이할 수도 있다.The plurality of discharge cells S may be all identical to each other, all may be different from each other, some may be the same, and others may be different.
또한, 상기 다수개의 토출용 셀(S)들은 크기가 모두 서로 동일할 수도 있고, 모두 서로 상이할 수도 있고, 일부는 동일하고 나머지 일부는 상이할 수도 있다.In addition, the plurality of discharge cells S may all have the same size, all may be different from each other, some may be the same, and others may be different.
본 발명에서는 상기 토출용 셀(S)의 크기 및 높이(h)를 특별하게 한정하지 않는다.In the present invention, the size and height h of the discharge cell S are not particularly limited.
본 발명에 따른 상기의 멀티-셀 타입 전기방사용 튜브는 전기방사용 튜브 지지체에 의해 지지되며, 전기방사용 튜브 하단에 위치하는 분배판을 통해 고분자 방사용액을 안정적으로 공급받는 것이 바람직하다.The multi-cell type electrospinning tube according to the present invention is supported by an electrospinning tube support, and it is preferable that the polymer spinning solution is stably supplied through a distribution plate located at the bottom of the electrospinning tube.
상기 전기방사용 튜브 지지체는 예를 들어 직경이 3㎜ 이상인 원통형 구조일 수도 있다.The electrospinning tube support may be, for example, a cylindrical structure having a diameter of 3 mm or more.
다음으로는 이상에서 설명한 본 발명의 멀티-셀 타입 전기방사용 튜브를 이용하여 나노섬유를 제조하는 방법에 대해 살펴본다.Next, a method of manufacturing nanofibers using the multi-cell type electrospinning tube of the present invention described above will be described.
본 발명에서는 고분자 방사용액을 전기방사용 튜브를 통해 전기방사하여 나노섬유를 제조할 때 정전기력과 원심력은 함께 이용할 수 있도록, 상기 전기방사용 튜브로서 원형 막대 및 다각형 막대 중에서 선택된 1종의 형태를 구비하는 다수개의 토출용 셀(S)들을 포함하는 멀티-셀 타입 전기방사용 튜브(T)를 사용하고, 전기방사시 상기 멀티-셀 타입 전기방사용 튜브(T)를 회전시켜 주는 것을 특징으로 한다.In the present invention, the electrospinning tube is provided with one type selected from a circular rod and a polygonal rod as the electrospinning tube so that the electrospinning and centrifugal force can be used together when the polymer spinning solution is electrospun through an electrospinning tube to produce nanofibers. A multi-cell type electrospinning tube T including a plurality of discharge cells S is used, and the multi-cell type electrospinning tube T is rotated during electrospinning. .
이때, 상기 멀티-셀 타입 전기방사용 튜브(T)의 회전수는 50rpm 이상, 보다 좋기로는 50~500rpm으로 설정해 주는 것이 바람직하다.At this time, the rotation speed of the multi-cell type electrospinning tube T is preferably set to 50 rpm or more, more preferably 50 to 500 rpm.
상기 멀티-셀 타입 전기방사용 튜브(T)의 회전수가 너무 낮으면 원심력도 낮아져 나노섬유 형성능이 떨어지게 되고, 상기 회전수가 너무 높으면 드롭발생현상이 일어나 바람지하지 못하다.If the number of revolutions of the multi-cell type electrospinning tube T is too low, the centrifugal force is also lowered, and the ability to form nanofibers is lowered.
그러나, 상기 멀티-셀 타입 전기방사용 튜브(T)의 회전수는 상기 전기방사용 튜브(T)에 형성된 셀(S)의 직경, 모양, 개수, 배열열수 및 배열방법 등에 따라 달라지므로 본 발명에서는 상기 회전수를 특별히 한정하는 것은 아니다.However, the number of rotation of the multi-cell type electrospinning tube (T) is different depending on the diameter, shape, number, arrangement number and arrangement method of the cell (S) formed in the electrospinning tube (T), the present invention In the above, the rotation speed is not particularly limited.
이하, 실시예를 통하여 본 발명을 보다 구체적으로 살펴본다.Hereinafter, the present invention will be described in more detail with reference to Examples.
그러나, 본 발명은 하기 실시예만으로 보호범위가 한정되는 것은 아니다.However, the present invention is not limited only to the following examples.
실시예 1Example 1
폴리비닐알코올(Aldrich, 미국) 100g을 증류수 900g에 용해하여 고분자 방사액을 제조한 다음, 도 1 및 도 3에 도시된 6각형 막대 형태이고 한변의 길이가 6㎜인 토출용 셀(S)들이 내경이 50㎜인 전기방사용 튜브(T)내에 벌집구조로 배열되어 있는 멀티-셀 타입 전기방사용 튜브(T)를 통해 전기방사(토출)하였다.After dissolving 100 g of polyvinyl alcohol (Aldrich, USA) in 900 g of distilled water to prepare a polymer spinning solution, discharge cells (S) having a hexagonal rod shape shown in FIGS. Electrospinning (ejection) was carried out through a multi-cell type electrospinning tube T arranged in a honeycomb structure in an electrospinning tube T having an inner diameter of 50 mm.
이때, 전기방사시 상기 멀티-셀 타입 전기방사용 튜브(T)를 200rpm으로 회전시켜 주었다.At this time, the multi-cell type electrospinning tube (T) was rotated at 200 rpm during electrospinning.
전기방사시 30kV의 전압을 상기 전기방사용 튜브와 컬렉터에 각각 걸어주었다.During electrospinning, a voltage of 30 kV was applied to the electrospinning tube and the collector, respectively.
상기 멀티-셀 전기방사용 튜브(T)를 통해 전기방사되는 나노섬유를 회전하는 컬렉터 상에 접적하여 나노섬유를 제조하였다.The nanofibers were prepared by contacting the nanofibers electrospun through the multi-cell electrospinning tube T on a rotating collector.
이때, 상기 멀티-셀 타입 전기방사용 튜브(T) 1개당 토출량은 0.5g/분으로서 종래 전기방사 장치의 토출량 대비 크게 향상되었다.At this time, the discharge amount per one of the multi-cell type electrospinning tube (T) is 0.5g / min, significantly improved compared to the discharge amount of the conventional electrospinning apparatus.
제조된 나노섬유 웹의 전자현미경 사진은 도 4와 같았으며 드롭발생 현상이 전혀 발생되지 않았다.The electron micrograph of the prepared nanofiber web was as shown in Figure 4 and no drop occurred.
제조된 나노섬유의 평균직경은 200㎚ 이였다.The average diameter of the prepared nanofibers was 200 nm.
실시예 2Example 2
폴리비닐알코올(Aldrich, 미국) 100g을 증류수 900g에 용해하여 고분자 방사액을 제조한 다음, 도 2에 도시된 8각형 막대 형태이고 한변의 길이가 4㎜인 토출용 셀(S)들이 내경이 50㎜인 전기방사용 튜브(T)내에 벌집구조로 배열되어 있는 멀티-셀 타입 전기방사용 튜브(T)를 통해 전기방사(토출)하였다.After dissolving 100 g of polyvinyl alcohol (Aldrich, USA) in 900 g of distilled water to prepare a polymer spinning solution, the discharge cells (S) in the form of an octagonal rod shown in FIG. Electrospinning (ejection) was carried out through a multi-cell type electrospinning tube T arranged in a honeycomb structure in an electrospinning tube T of mm.
이때, 전기방사시 상기 멀티-셀 타입 전기방사용 튜브(T)를 200rpm으로 회전시켜 주었다.At this time, the multi-cell type electrospinning tube (T) was rotated at 200 rpm during electrospinning.
전기방사시 30kV의 전압을 상기 전기방사용 튜브와 컬렉터에 각각 걸어주었다.During electrospinning, a voltage of 30 kV was applied to the electrospinning tube and the collector, respectively.
상기 멀티-셀 전기방사용 튜브(T)를 통해 전기방사되는 나노섬유를 회전하는 컬렉터 상에 접적하여 나노섬유를 제조하였다.The nanofibers were prepared by contacting the nanofibers electrospun through the multi-cell electrospinning tube T on a rotating collector.
이때, 상기 멀티-셀 타입 전기방사용 튜브(T) 1개당 토출량은 0.55g/분으로서 종래 전기방사 장치의 토출량 대비 크게 향상되었다.At this time, the discharge amount per one of the multi-cell type electrospinning tube (T) is 0.55g / min, significantly improved compared to the discharge amount of the conventional electrospinning apparatus.
제조된 나노섬유 웹에는 드롭발생 현상이 전혀 발생되지 않았다.No drop occurred in the fabricated nanofiber web.
제조된 나노섬유의 평균직경은 210㎚ 이였다.The average diameter of the prepared nanofibers was 210 nm.
실시예 3Example 3
폴리비닐알코올(Aldrich, 미국) 100g을 증류수 900g에 용해하여 고분자 방사액을 제조한 다음, 도 1 및 도 3에 도시된 6각형 막대 형태이고 한변의 길이가 6㎜인 토출용 셀(S)들과 도 2에 도시된 8각형 막대 형태이고 한변의 길이가 4㎜인 토출용 셀(S)들이 교호로 반복되게 내경이 50㎜인 전기방사용 튜브(T)내에 벌집구조로 배열되어 있는 멀티-셀 타입 전기방사용 튜브(T)를 통해 전기방사(토출)하였다.After dissolving 100 g of polyvinyl alcohol (Aldrich, USA) in 900 g of distilled water to prepare a polymer spinning solution, discharge cells (S) having a hexagonal rod shape shown in FIGS. 1 and 3 and having a length of 6 mm on one side are shown. 2 is arranged in a honeycomb structure in an electrospinning tube T having an inner diameter of 50 mm so that the discharge cells S having a length of 4 mm on one side are alternately repeated. It was electrospun (discharged) through the cell type electrospinning tube (T).
이때, 전기방사시 상기 멀티-셀 타입 전기방사용 튜브(T)를 200rpm으로 회전시켜 주었다.At this time, the multi-cell type electrospinning tube (T) was rotated at 200 rpm during electrospinning.
전기방사시 30kV의 전압을 상기 전기방사용 튜브와 컬렉터에 각각 걸어주었다.During electrospinning, a voltage of 30 kV was applied to the electrospinning tube and the collector, respectively.
상기 멀티-셀 전기방사용 튜브(T)를 통해 전기방사되는 나노섬유를 회전하는 컬렉터 상에 접적하여 나노섬유를 제조하였다.The nanofibers were prepared by contacting the nanofibers electrospun through the multi-cell electrospinning tube T on a rotating collector.
이때, 상기 멀티-셀 타입 전기방사용 튜브(T) 1개당 토출량은 0.6g/분으로서 종래 전기방사 장치의 토출량 대비 크게 향상되었다.At this time, the discharge amount per one of the multi-cell type electrospinning tube (T) is 0.6g / min, significantly improved compared to the discharge amount of the conventional electrospinning apparatus.
제조된 나노섬유 웹에는 드롭발생 현상이 전혀 발생되지 않았다.No drop occurred in the fabricated nanofiber web.
제조된 나노섬유의 평균직경은 205㎚ 이였다.The average diameter of the prepared nanofibers was 205 nm.
본 발명은 품질이 우수한 나노섬유를 높은 생산성으로 전기방사하는 장치로 이용된다.The present invention is used as a device for electrospinning high quality nanofibers with high productivity.

Claims (8)

  1. 원형 막대 및 다각형 막대 중에서 선택된 1종의 형태를 구비하는 다수개의 토출용 셀(S)들로 구성되는 것을 특징으로 하는 멀티-셀 타입 전기방사용 튜브.Multi-cell type electrospinning tube, characterized in that consisting of a plurality of discharge cells (S) having one type selected from a circular bar and a polygonal bar.
  2. 제1항에 있어서, 다수개의 토출용 셀(S)들 각각의 높이(h)가 서로 동일한 것을 특징으로 하는 멀티-셀 타입 전기방사용 튜브.The multi-cell type electrospinning tube according to claim 1, wherein the height h of each of the plurality of discharge cells S is the same.
  3. 제1항에 있어서, 다각형 막대 형태인 토출용 셀(S)은 모서리 각이 3개~16개인 것을 특징으로 하는 멀티-셀 타입 전기방사용 튜브.The multi-cell type electrospinning tube according to claim 1, wherein the discharge cells (S) having a polygonal bar shape have 3 to 16 corner angles.
  4. 제1항에 있어서, 다수개의 토출용 셀(S) 각각의 형태 및 크기가 모두 서로 동일한 것을 특징으로 하는 멀티-셀 타입 전기방사용 튜브.The multi-cell type electrospinning tube according to claim 1, wherein the shape and size of each of the plurality of discharge cells S are the same.
  5. 제1항에 있어서, 다수개의 토출용 셀(S) 각각의 형태 및 크기가 모두 서로 상이한 것을 특징으로 하는 멀티-셀 타입 전기방사용 튜브.The multi-cell type electrospinning tube according to claim 1, wherein the shape and size of each of the plurality of discharge cells S are different from each other.
  6. 제1항에 있어서, 다수개의 토출용 셀(S)중 일부는 형태 및 크기가 서로 동일하고, 나머지 일부는 형태 및 크기가 서로 상이한 것을 특징으로 하는 멀티-셀 타입 전기방사용 튜브.The multi-cell type electrospinning tube according to claim 1, wherein some of the plurality of discharge cells S have the same shape and size, and others have different shapes and sizes.
  7. 고분자 방사용액을 전기방사용 튜브를 통해 전기방사하여 나노섬유를 제조함에 있어서, 상기 전기방사용 튜브로서 원형 막대 및 다각형 막대 중에서 선택된 1종의 형태를 구비하는 다수개의 토출용 셀(S)들을 포함하는 멀티-셀 타입 전기방사용 튜브(T)를 사용하고, 전기방사시 상기 멀티-셀 타입 전기방사용 튜브(T)를 회전시켜 주는 것을 특징으로 하는 멀티-셀 타입 전기방사용 튜브를 이용한 나노섬유의 제조방법.In manufacturing a nanofiber by electrospinning a polymer spinning solution through an electrospinning tube, the electrospinning tube includes a plurality of discharge cells (S) having one type selected from a circular rod and a polygonal rod. Using a multi-cell type electrospinning tube (T) and rotating the multi-cell type electrospinning tube (T) during electrospinning. Method of making fibers.
  8. 제7항에 있어서, 전기방사시 상기 멀티-셀 타입 전기방사용 튜브를 50rpm 이상으로 회전시켜 주는 것을 특징으로 하는 멀티-셀 타입 전기방사용 튜브를 이용한 나노섬유의 제조방법.The method of manufacturing nanofibers using the multi-cell type electrospinning tube according to claim 7, wherein the multi-cell type electrospinning tube is rotated at 50 rpm or more during electrospinning.
PCT/KR2013/006476 2013-07-19 2013-07-19 Multi-cell type electrospinning tube and method for producing nanofibers using same WO2015008883A1 (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060009511A (en) * 2004-07-26 2006-02-01 김학용 Methods of manufacturing for high strength filament with nanofibers
KR20070100481A (en) * 2006-04-07 2007-10-11 주식회사 코오롱 Spinning die for lyocell fibers, and method for preparation of lyocell fibers by using the same
KR20110079249A (en) * 2009-12-31 2011-07-07 주식회사 효성 Melt electrospinning device and multi-nozzle block for the same
KR101118079B1 (en) * 2008-08-08 2012-03-09 코오롱패션머티리얼 (주) Method of manufacturing nanofiber web
KR20130026207A (en) * 2011-09-05 2013-03-13 전북대학교산학협력단 Multi-cell type electrospun tube and method of manufacturing nano fiber thereby

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060009511A (en) * 2004-07-26 2006-02-01 김학용 Methods of manufacturing for high strength filament with nanofibers
KR20070100481A (en) * 2006-04-07 2007-10-11 주식회사 코오롱 Spinning die for lyocell fibers, and method for preparation of lyocell fibers by using the same
KR101118079B1 (en) * 2008-08-08 2012-03-09 코오롱패션머티리얼 (주) Method of manufacturing nanofiber web
KR20110079249A (en) * 2009-12-31 2011-07-07 주식회사 효성 Melt electrospinning device and multi-nozzle block for the same
KR20130026207A (en) * 2011-09-05 2013-03-13 전북대학교산학협력단 Multi-cell type electrospun tube and method of manufacturing nano fiber thereby

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